Standard Reference Materials : the first century€¦ · NIST260-150...

NIST 260-150

Standard Reference Materials - The First Century

Stanley D. Rasberry, AuthorTomara Arrington, Composition and Design

Standard Reference Materials ProgramTechnology Services

National Institute of Standards and Technology

Gaithersburg, MD 20899-2320

January 2003

U.S. Department of CommerceDonald L. Evans, Secretary

Technology Administration

Phillip J. Bond,

Under Secretary of Commerce for Technology

National Institute of Standards and Technology

Arden L. Bement, Jr., Director

Please visit our website

WWW.n ist.gov/srm

Forewordstandard Reference Materials have played a major role in the history of the National Institute of

Standards and Technology (NIST), as well as its predecessor organization, the National Bureau of

Standards (NBS). Standard Reference Materials (SRMs) were one of the first tangible outputs fromthe nation's investment in improved measurement standards and technology that was started at

the beginning of the 20th century. As both NBS/NIST evolved over the last hundred years in termsof scientific capability and fields of work, SRMs have taken on new forms and new roles in ensur-

ing that our Nation is second to none in measurement capability.

No one is more familiar with the history of this important program than Stanley Rasberry, long-

time Chief of the program as well as a major developer of SRMs himself. In this retrospective,

Rasberry captures the spirit and importance of the program for analysts, researchers and technolo-

gists everywhere. The reader will find this lively exposition both informative and enlightening

about one of NIST's most important programs.

John RumbleJanuary 2003

Acknowledgment

The Author wishes to acknowledge the fine contributions of Nancy Trahey-Bale and Lee Best for

their assistance in preparing this document.

standard Reference Maten^is i ne First Century

The entire charge to the new agency was

found in six provisions:

• custody of the standards;

• comparison of the standards used in scien-

tific investigations, engineering, manufac-

turing, commerce, and educational insti-

tutions with the standards adopted by or

recognized by the Government;

• construction, when necessary, of stan-

dards, their multiples and subdivisions;

• testing and calibration of standard meas-

uring apparatus;

• solution of problems which arise in con-

nection with standards; and,

• determination of physical constants and

the properties of materials, when such

data are of great importance and are not

to be obtained of sufficient accuracy else-

where.

The Bureau could have emerged at no more

opportune time. It was the dawn of virtually

every technology that we know today - auto-

mobiles, airplanes, modern ships and locomo-

tives, steel construction, motion pictures,

practical radio, and subsequently, television,

space craft, computers, and information tech-

nology. In the early days, the Bureau was

"right in the middle" of every one of these

fields. As we shall see, analytical chemistry

had a role in most.

The need to be relevant frequently directed

the early work in analytical chemistry to top-

ics where materials simply were not

up to the challenging

new applica-

tions. With these enormous needs in mind,

the Congress of the United States gave care-

ful deliberation to the staffing of the newBureau. Initially, it decided it would not be

sufficient to have a director, a physicist and

two assistant physicists; a chemist and two

assistant chemists also would be allocated.

Later, in 1901, the expense of constructing

the new laboratory and the scarcity of funds

caused the Congress to cancel the two assis-

tant chemist positions. Thus in its first year,

the young agency began trade-offs between

staff and facilities that last to this day.

An Urgent NeedMany of the greatest technical challenges of

the early twentieth century were related to

materials and their performance.

Construction of skyscrapers and suspension

bridges would require new and stronger

alloys of steel, and better quality control for

Portland cement used in concrete. Tungsten

alloy performance would become critical to

vacuum tubes for lighting and electronics.

Copper alloys would figure heavily in wiring

for communications and in valves and fittings

with nearly endless configurations.

Perhaps the material concerns were nowhere

more critical than in the automotive fields.

Practical automobiles and aircraft were on

the threshold - they needed an

array of new materials

ranging

2 Standard Reference Materials - The First Century

from nodular cast irons to

high strength aluminum alloys

to specialized rubber to carefully

tempered glass. New and vastly larger

ships were on the drawing boards - they

needed new alloys of corrosion resistant

steel, monel, bronze, and many other

improved materials.

could help |- .

with ques- - ". • . • ^ -

tions of laboratory ' -^"^internal consistency but shed little lighfon

analytical disagreements among several labo-

ratories. Methods were practically limited to

those based immediately on first principles

where standards could be physical. This still

left open questions of completeness of sepa-

ration, stoichiometry, purity of reagents, and

other issues. Evaluating the accuracy of newly

emerging instrumental methods would pro-

duce even greater need for certified reference

materials to serve, first as accuracy bench-

marks, and then as calibrators for quality assur-

ance into the future.

The Bureau accepted the challenge and set to

work - but not alone. In fact, this very first

reference material project set a precedent for

cooperative efforts that continue to this day.

Included in that precedent is the idea that

projects will be started only on demonstrated

need and demand of the technical communi-

ty. Furthermore, priority will be assigned to

those projects where cooperation of the

requesters is assured. This has helped the

Bureau select worthy projects over the years.

The cooperation has included provision or

preparation of materials and contribution of

data to the certification campaign. In the

case of the first ever project, cooperation

with the American Foundrymen's Association

extended to all three of these aspects. The

Railroad trains had already increased the

speed of overland transport by an order of

magnitude, but not without the cost of manylives due to material failures. The first pas-

senger fatality had occurred in 1833, near

Heightstown, NJ. Former president John

Quincy Adams and Cornelius Vanderbilt were

aboard the train, but not injured. Preventing

future loss of lives was an urgent need that

pressed the Bureau into the new venture of

certifying reference materials.

In 1905, the American Foundrymen's

Association approached the Bureau to see if

it would assume leadership of a new work

the Association had recently begun. The

Association was trying to solve the problem

of rail car derailments due to the fracturing

of cast iron wheels. Appropriate alloys had

been found and Association research showed

that they would cure the problem. However,

the chemical laboratories at the various

foundries that supplied materials to the rail-

roads could not analyze the materials with

sufficiently consistent accuracy to provide

ongoing quality assurance. The problem as

the foundrymen defined it was to have a

source of accurately analyzed materials hav-

ing compositions at and bracketing the com-

positions of alloys known to be acceptable.

Those "standardizing" materials could then

be used by the foundries to maintain their

analyses in control.

At the time, chemists throughout the world

were expected to develop and maintain their

own lots of materials that could be used as

benchmarks for calibrating or testing analyses.

Standard Reference Materials - The First Century 3

When the first project was completed in

1906, four materials were placed on sale

together with their certificates of analyses to

serve as the needed benchmarks. They con-

sisted of bottles of cast iron chips which were

labeled "Standardizing Iron Sample A,"

through "Standardizing Iron Sample D."

Their worth was quickly realized in improved

cast iron rail car wheels and an improved

safety record for the railroads.

analytical work was carried out in several

companies that were members of the

Association, and the Association provided to

the Bureau an industrial research associate to

do the analytical work at NBS. The young

chemist, John Cain, would become a full

member of the staff, about twenty years

later.

certification campaigns were required to pro-

vide new certificates of analysis. Also differ-

ent was the labeling system. By the time the

second lots were prepared, the cast irons

were part of a larger program of reference

materials, which by about 1910, had become

known as "Standard Samples."

"Standardizing Iron Sample B" became

"Standard Sample No. 4a - Iron B." The num-

bers 3, 4, 5, and 6 were never assigned with-

out the "a" designation, owing perhaps to

the originals having been issued with letter

designations. Standard sample numbers 1

and 2 had been assigned to other materials,

so they were not available to the cast irons.

Two of the original formulations of cast iron

have been renewed at every exhaustion

since. For Cast Iron C, there have now been

14 lots prepared over the past 95 years.

When the initial lots of materials were

exhausted, they were replaced with new lots

of nearly equal composition. Of course the

new lots were slightly different, thus new

Success inspires imitation

The success of the cast iron reference materi-

als led to expansion of the concept into newmaterial types. Certification work on several

other alloys, iron

standard Reference Material (SRM) 5m is ttie fourteenth lot (thirteenth renewal) of

Standardized Iron Sample C, and has in recent years, been certified in cooperation

with ASTM. Note the "C" designation has been dropped.

ores, and copper

slags began the

same year as the

cast irons were

issued. All these

activities caught

the interest of the

steel producers. Amember of the

Bureau's Visiting

Committee, Albert

Ladd Colby, was a

leading authority

on metallurgy, and

he urged the

Bureau to extend

its success with cast

iron into the field

of steel. Perhaps

because it was

smaller then, the

Bureau was quite


agile in starting new projects and new coop-

erative ventures. It was able to start this neweffort together with the Association of

American Steel Manufacturers in 1907. Aseries of 17 steel standard samples emerged

and set NBS-NIST on a path of support to the

U.S. steel industry that has spanned nine

chemical analysis. More importantly, the

interest of the Nation's chemists was growing

too, with observation of the utility of the

"Standard Samples" wherever they were

available. Clearly, more types of materials

would be needed, and they were on the waywith the cooperation of the American

ChemicalSociety, and

sk^ later the

PortlandCementAssociation,

the Copper

Table 1. The First 14 Metal Reference Materials and their First Renewals (with numbers)

Standardized Iron Sample A 1906 Standardized Steel Bessemer 0.4 1907

ss 3 White Iron 1958 SS 10a Bessemer Steel 0.4 % C 1911

Standardized Iron Sample B 1906 Standardized Steel B.O.H. 0.2 1908

ss 4a Cast Iron B 1910 SS 11a Basic Open Hearth Steel 0.2 % C 1911

Standardized Iron Sample C 1906 Standardized Steel B.O.H. 0.4 1908

ss 5a Cast Iron C 1910 SS 12a Basic Open Hearth Steel 0.4 % C 1911

Standardized Iron Sample D 1906 Standardized Steel B.O.H. 0.6 1908

ss 6a Cast Iron D 1910 SS 13a Basic Open Hearth Steel 0.6 % C 1911

ss 7 Iron E 1917 Standardized Steel B.O.H. 0.8 1908

ss 7b Cast Iron (High Phosphorus) 1926 SS 14a Basic Open Hearth Steel 0.8 % C 1911

Standardized Steel Bessemer 0.1 1907 Standardized Steel B.O.H. 0.1 1908

ss 8a Bessemer Steel 0.1 % C 1911 SS 15a Basic Open Hearth Steel 0.1 % C 1911

Standardized Steel Bessemer 0.2 1907 Standardized Steel B.O.H. 1.0 1908

ss 9a Bessemer Steel 0.2 % C 1911 SS 16a Basic Open Hearth Steel 1.0 % C 1911

decades. At the beginning of the effort, the

chief of the Chemistry Division was Dr.

William Noyes, and the analytical work at the

Bureau was done by John Cain and three

other chemists: Witmer, Isham, and Waters,

all of whom were probably industrial

research associates.

By 1911, the catalog of reference materials

had grown to 25 entries, all in support of

Development Association, and numerous

other groups.

The Early Catalog

While the new concept of standard samples

was sure to expand to many new types, that

expansion did not produce a rational num-

bering system. From 1906 until 1910, num-

bers were not assigned, and the term stan-

dard sample was not used. To help examine

Standard Reference Materials - The First

Tab[e 2. Other Examples Selected From the First 100 Standard Sample Numbers

SS 1 Argillaceous Limestone 1910 SS 43 Zinc (M.P. or F.RCirc.66) 1915?

SS 2 Zinc Ore 1919 SS 44 Aluminum (M.P. or F.R Circ.66) 1915?

SS 17 Sucrose (Stoichiometry) 1912 SS 45 Copper (M.R or F.RCirc.66) 1915?

SS 19-23 A series of carbon steels 1910 - 1920 SS 46 Portland Cement Sieve Test 1915?

SS 24 Vanadium Steel 0.15 % V 1910 SS 47 Portland Cement Sieve Test 1915?

SS 25 Manganese Ore 1910 SS 48 Benzoic Acid (Acidimetric) 1919?

SS 26 Crescent Iron Ore 1910 SS 49 Lead (Freezing Point) 1915?

SS 27 Sibley Iron Ore 1910 SS 50 Cr - W - V Steel 1921

SS 28 Norrie Iron Ore 1910 SS 52 Cast Bronze 1921

SS 29 Magnetite Iron Ore 1910 SS 53 Lead-base Bearing Metal 1921

SS 30 Chrome-Vanadium Steel 1912 SS 54 Tin-base Bearing Metal 1923

SS 31 Chrome-Tungsten Steel 1912 SS 57 Silicon Metal 1924

SS 32 Chrome-Nickel Steel 1912 SS 58 Ferrosilicon 1924

SS 37 Sheet Brass 1914 SS 60 Ferrovanadium 1924

SS 38 Napthaiene (Heat of Combustion) 1912 SS 80 Soda-lime Glass 1927

SS 39 Benzoic Acid (Heat of Comb.) 1912 SS 83 Arsenic Trioxide(Reductiometric) 1927

SS 40 Sodium Oxalate (Oxidimetry) 1924 SS 85 Aluminum Alloy (Duralumin) 1943

SS 42 Tin (M.P. or F.P.Circ.66) 1915? SS 98 Plastic Clay 1931

some of the materials comprising the first 100

certified, two tables are presented. In Table

1, the initial 14 metal reference materials are

listed, together with the designations of their

first renewals. Table 2 lists other examples

drawn from the first 100 standard sample

numbers.

It is not clear that SS 7 Iron E was ever pro-

duced as a "Standardized Iron E." The earli-

est available certificate is for SS 7 without an

"a" designation, indicating that it may repre-

sent the first time the material was pro-

duced. Other metal standard samples

were produced in the 1910 to 1912 time peri-

od, as is indicated in Table 2. It is also inter-

esting to note that the elapsed time before

first renewal was typically only three to four

years, indicating heavy usage.

It is not surprising that limestone was an

early standard sample - it was useful as a

refractory liner in metals production. The

first material to be certified that was com-

pletely unrelated to metal production was

sucrose as a calibrating material for polarime-

ters. "SS 2" was reserved for zinc ore as early

as 1910, although the first archived certifi-

cate is dated 1919. Early additions to the cat-

alog included primary chemicals to assist In

calibrating titrations, and several standard

samples for physical chemistry, especially for

calibrating calorimeters and thermometers.

From the information in Table 2, it would

appear that there was a slowing of reference

material production during World War I. At

the time significant portions of the Bureau


Table 3. NBS Programs and Staff (Noting Source of University Degree) - June 1904

Division I - Weights & Measures, Thermometry, Optics, Engineering Instruments

Louis Fischer Columbia University

Llewelyn Hoxton University of Virginia

Roy Ferner University of Wisconsin

Nathan Osborne Michigan School of Mines

Charles Waidner Johns Hopkins University

George Burgess University of Paris

Hobart Dickinson Clark University

Samuel Stratton University of Illinois

Frederick Bates University of Nebraska

Perley Nutting Cornell University

Albert Merrill Massachusetts Institute of Technology

Weights & MeasuresWeights & Measures

Weights & Measures

Weights & MeasuresHeat & ThermometryHeat & ThermometryHeat & ThermometryOptics + Director. NBSOptics

Optics

Engineering Instruments

Division II - Electricity

Frank Wolff

Francis CadyGeorge Middiekauf

Karl GutheEdward Rosa

Ernest Dorsey

Frederick Grover

Morton Lloyd

Herbert Brooks

C. E. Reid

Franklin Durston

Edward HydeCharles Sponsler

Johns Hopkins University

Massachusetts Institute of Technology


University of Michigan

Wesleyan University


Wesleyan University

University of Pennsylvania

Ohio State University

Purdue University

Wesleyan University


Pennsylvania State College

Resistance & EmfResistance & EmfResistance & EmfMagnetism & Absolute Current

Inductance & Capacity



Electrical measuring instruments




Photometry

Engineering Plant

Division III - Chemistry

William NoyesHenry Stokes



staff were redirected to the war effort, a pre-

cursor to the much larger dedication of per-

sonnel (approximately 4000) to supporting

the military in World War II. Shortly after the

first war, "SS 85" was reserved for the alu-

minum alloy "Duralumin" even though it was

not certified until 1943.

An Unintended Consequence of

Success in Reference Materials

The early work on Standard Samples at the

Bureau had a profound impact on the later

work of the agency. The U.S. Congress had

initially seen the agency as being primarily

dedicated to construction and maintenance

of the physical standards of measurement. It

seems quite clear that by looking at the ear-

liest staff and their work of the Bureau (see

Table 3), that there was no plan to emphasize

studies in chemical and material fields further

than what was needed to support programs

in instrumentation and metrology.

Despite the initial lack of agency emphasis on

materials efforts, the great success of the

Standard Samples work weighed heavily in

steering most of the growth of the newagency into the direction of solving practical

material problems and, in some cases, using

cutting edge instrumentation and methods.

Later amendments to the agency's organic

act recognized the Bureau's contributions to

materials characterization and development,

and by 1950 provided specific authority to

certify and distribute reference materials as

the leading U.S. authority.

Standard Reference Materials tury 7

.....^ Domestic Industries

Research at the Bureau occasionally provided

initiative for the production of a new SRM,

and very often provided the tools needed to

certify materials with a reduced uncertainty.

There are also cases where the production of

an SRM inspired the start of an industry newto the United States. A striking example of

that occurred during World War I. Before

that war, the Bureau was distributing stan-

dard samples of sugar for three important

applications: calibrating saccharimeters; cali-

brating calorimeters used in measuring the

heat content of fuels; and for use in differen-

tiating bacteria in medical laboratory tests.

Germany was the source of the pure sugars

that the Bureau characterized, certified, and

sold.

When the war broke out and the materials

were no longer available, the Bureau had to

produce its own pure sucrose and dextrose.

The German patents and production litera-

ture were written so obliquely to protect pro-

prietary rights from other producers that

reconstruction of the production processes

required almost completely original research.

The results were well worth the effort

because the output was not only Bureau

Standard Samples, but also the technology

for producing low cost dextrose that

launched a new domestic industry for

American sugar producers and corn farmers.

William Meggers applied

spectroscopy to physical andchemical measurements.

The connection with instrument manufactur-

ers is perhaps less direct; but nevertheless,

just as real. The ideas developed at the

Bureau to solve all manner of analytical prob-

lems were frequently blended with the work

of instrument makers to either create newinstruments or impact the progress in devel-

opments of existing ones. Perhaps the tradi-

tion started with recruitment from 1901 to

1904 of the first 26 professional staff mem-bers, seven of whom were from the Johns

Hopkins University. Johns Hopkins was at the

time an international leader in spectroscopic

technology, so perhaps it was fitting that the

entire Chemistry Division professional staff of

two were from Hopkins - William Noyes and

Henry Stokes. It was Noyes who first pro-

duced atomic mass data at the Bureau,

reporting in 1907 the mass of atomic weigh-

ing of several elements, including hydrogen

at 1.00783.

In 1905, William Coblentz joined the staff

and would serve the Bureau for the next 40

years. By 1914, William Meggers had also

come from Johns Hopkins to join the staff,

and would contribute for 52 years to a wide

variety of spectroscopic techniques that

would later find their way into commercial

production.

Just as many of the early instrumental tech-

niques for chemical analysis found their basis

in spectroscopy, so grew the need for refer-

ence materials. This resulted from most spec-

trochemical techniques requiring reference

materials as calibrants.

Early Connections - Lasting Patterns

One of the most interesting aspects found in

studying the early technical efforts of the


The Challenger

flight STS-6

provided

(National

Aeronautics

and Space

Administration)

the 10pm

spheres for

SRM 1960.

Bureau is the degree to which they estab-

lished enduring programs of reference mate-

rial production. Some of these cases are so

obvious as to require no further explication,

for example the program in cast iron stan-

dard samples setting a 95-year-long pattern

that lasts to the present. Some others are less

obvious but no less interesting:

Radioactivity - In 1911 Marie Curie pre-

pared the first standard for activity as a

sealed glass tube containing weighed

amounts of radium and radium salts and

characterized for its gamma ray count rate.

The standard was accepted as an interna-

tional standard and was maintained at the

BIPMi France. A similar tube was prepared

and calibrated with the one at BIPM for

delivery to the Bureau in 1913, becoming

our Nation's first standard for radioactivity.

This would serve as the start of a program

that would see the Bureau develop refer-

ence materials to accommodate every

aspect of radioactivity measurement.

An interesting repayment occurred in 1921

for Mme. Curie's earlier generosity to the

scientific community. By that time, she was

in need of additional radium to pursue her

investigations, but the material was too

expensive for her resources. On hearing of

her plight, a group of American womenbanded together and raised the funds nec-

essary to purchase 1g of radium for Mme.Curie. The material was certified by the

Bureau for purity and activity and was pre-

sented to the famous scientist by President

Warren Harding.

Today, NIST has more than 70 radioactivity

SRMs in the catalog. These cover a wide

range of applications, including certified

activity for radiopharmaceuticals, alpha

particle point sources, and gamma ray

point sources.

Aviation/NASA - From the first days of

aviation, NBS took an active part in devel-

oping the technology. Wind tunnels were

quickly constructed to develop improved

dii- airfoils and a special laboratory building

srn (the Dynamometer Building) was con-

ess structed to research the weakest link in the

whole enterprise, the engines. Absolutely

the highest power-to-weight ratio was

needed, and that meant higher compres-

sion and extreme demands on fuels.

Reference materials were issued for isooc-

tane and n-heptane to serve as quality con-

trols for the emerging aviation fuel indus-

try. Calorimetry reference materials were

vital in designing the best fuels for piston,

jet and rocket engines.

trots for

try. Cal<

vital in c

jet and r

In 1915 the National Advisory Committee

for Aeronautics (NACA) was formed; the

Bureau had a leading place in the commit-

tee. The other agencies, including the

Army and Navy, did not have aeronautical

facilities, so the laboratory work fell to the

Bureau. In late 1932, President-elect

Roosevelt proposed folding NACA into the

Bureau. That proposal was never carried

out, but in 1946 Hugh Dryden, one of the

nation's top theoretical aerodynamicists,

left the Bureau to direct all research at

NACA. He subsequently led the transfor-

mation of NACA into NASA in 1958.

Later, reference materials of many types

contributed to aerospace development.

Aluminum alloys, and high-strength alloys

were needed for skins and airframes. High

temperature alloys were needed for jet

and rocket engine hot-section compo-

nents. NDE (non-destructive evaluation)

reference materials were needed for moni-

toring part reliability in service. Every ref-

erence material in support of electronics

technologies has a carry-over application in

The Bureau International des Poids and Measures (BIPM) is located in Sevres, a suburb of Paris. It has the task

of ensuring worldwide unifacation of physical measurements.


In the mid-1980s, the Standard Reference

Materials Program organized the certifica-

tion campaign for the first commercialized

material produced in space - a length stan-

dard at microscopic scale. Perhaps it was

the long-term connections between the

two agencies that gave NASA the confi-

dence in NBS to carry out the novel project.

The material certified was SRM 1960

Nominal 10 pm Diameter Polystyrene

Spheres (certified as 9.89 [sm ± 0.04 pm).

John Vanderhoff of Lehigh U. and Dale

Kornfeld of NASA had teamed together to

produce spheres in "Monodisperse Latex

Reactors" aboard five missions in 1982 and

1983. The missions were STS 3-4 and STS 6-

8, with the spheres for SRM 1960 being

produced aboard the Challenger's STS 6

mission. After the Challenger disaster,

George Uriano (SRM chief, 1979 - 1983)

served as a Congressional staff member in

the investigation of the tragedy.

Forensic "Signatures" - Just as one could

say that NASA was a Bureau spin-off, the

same is true for the crime laboratory at the

Federal Bureau of Investigation (FBI).

The FBI had no crime

lab prior

to 1932, when the Bureau assisted in its

development. Before that time, the

Bureau did laboratory work as a service to

the FBI, including the famous Lindbergh

kidnapping case in 1932. The Bureau had

significant impact on the case through the

handwriting analysis of Wilmer Souder

who conducted forensic investigations for

the Bureau from 1913 until 1954.

Most forensic signatures are not in hand-

writing. Perhaps more important are bul-

let lead markings, broken glass matching,

breathalyzer tests, drugs of abuse in urine,

and DNA profiling. Over the past 60 years,

NBS/NIST has certified reference materials

for all these signatures.

Proximity Fuse/Electronics - A major

NBS contribution to the ordinance effort

for World War II was the development of

the proximity fuse that caused shells and

bombs to explode at a predetermined

point above the ground. By the 1950s, all

such direct military work was transferred

out of the agency. However, a great deal

of the technical work associated with the

fuses was to miniaturize and harden the

associated electronic circuitry. The funda-

mental parts of that work stayed at NBS

and stimulated the development of a

number of SRMs.

Today, the SRMs related to electronics

cover a wide array, from the composition

of solder alloys to the transmission proper-

ties of complex optoelectronic devices.

Perhaps most basic are those for the con-

ductivity and resistance of a variety of met-

als and, especially, silicon. Residual resistiv-

ity ratio SRMs are also available for silicon.

Dimensional metrology is so critical to

semiconductor manufacture quality assur-

ance that NIST has developed photomask

linewidth artifacts, such as SRM 475, for

calibrating optical and scanning electron

microscopes, and has developed a range of

thin film thickness SRMs for ellipsometry.

he First Century

Highways for a Nation - When Dwight

Eisenhower became president in 1953,

one of his programs was to link every part

of the Nation with a modern high-speed

highway network, the Interstate Highway

System. The Bureau of Public Roads at the

time had no laboratory, so it funded sig-

nificant levels of work at NBS, including

efforts on Portland cement that would

eventually be organized as the Concrete

and Cement Research Laboratory. Field

laboratories for testing concrete were

maintained in San Francisco, CA;

Riverside, CA; Denver, CO; Alientown, PA;

and, Seattle, WA in addition to the main

NBS facility at Connecticut Avenue and

Van Ness Street, in Washington, D.C.

What remains at NIST today are the complex

metrology issues associated with health-

related measurements in such areas as the

environment, clinical chemistry, pharmaceuti-

cal measurements, food labeling, and nutri-

tional studies. The general SRM categories

for these are listed in Table 7. For these

fields, NIST has excelled in providing hun-

dreds of well-selected and characterized

SRMs. Environmental natural matrix materi-

als are covered with a wide variety of solids,

liquids, and gases being covered for both

inorganic and organic con-

stituents. More than 35 differ- ^ent SRMs serve to validate clin-

ical laboratory determina-

tions. Most analytical instru-

ments found in pharmaceuti-

cal laboratories have one or

more SRMs available to pro-

vide measurement trace-

ability. Some of the newest BHHlHSRM work has been dedicat- iLged to food analysis, with kS^^about 30 types of applicable 1^SRMs now available. >

The quality of the roads constructed would

rest in part on the accuracy with which the

Portland cement was formulated to meet

local gravel, temperature, and humidity

conditions. NBS already had experience

with Portland cement reference materials,

so the highway program provided need

and opportunity to expand the SRM cata-

log with more than a dozen new offerings

for cement composition, particle size, and

rheology.

Consumer Protection/Health - While the

Bureau has produced many services and

publications of interest to consumers, it has

never been primarily a consumer products

laboratory. Indeed, if described beyond

being a metrology laboratory, the more

comfortable niche would be as an industri-

ally-oriented laboratory. When the

Consumer Product Safety Commission

(CPSC) was formed in the 1960s, it had no

laboratory and depended entirely upon

NBS for laboratory support. During the

1970s, the level of work had increased suf-

ficiently that CPSC could start its own labo-

ratory with the help and transfer of many

NBS staff members.

A Team Approach - From

the earliest days of coop-

eration with the American

Foundrymen's Association, the 'sj^

Bureau has built on the success of

steady growth in cooperation with techni-

cal societies and standards organizations.

Perhaps no part of Government is as wel-

come in the activities of such bodies. This

means NIST is usually the agency most

likely to be trusted as an "honest techni-

cal broker" of ideas and programs. Even a

partial list of cooperating organizations

would need to include the American

Society for Testing and Materials (ASTM)

International, the Society of Automotive

Engineers (SAE), the Institute for Electrical

and Electronic Engineering (IEEE), the

' REFERENCE MATERIA

2383 ^Baby FoodComposite

^ ffi ip.^' i ANn.VKUS .VND TECHM>1

^THERSBUKi;. Ml) 208SW

Standard Referen The First Century 11

American Chemical Society (ACS), the

American Ceramic Society (ACS), the

Institute for Textile and Color Chemists

(ITCC), the American Iron and Steel

Institute (AISI), the Copper Development

Association (CDA), the College of American

Pathologists (CAP), and the American

Association of Clinical Chemistry (AACC).

NIST has had joint programs to develop or

share SRMs with every one of these organ-

izations and many more besides. See

Appendix A.

Continuing Efforts

Between the two World Wars, Standard

Sample activities grew slowly, but steadily.

Industrial needs for materials for chemical

analysis were the major, almost exclusive,

impetus. Starting in World War II the needs

for Standard Samples began to grow and

change.

As a primary national laboratory for mate-

rials research, NBS contributed to the

Manhattan Project through uranium

studies. Among other accomplish-

ments, NBS scientists carried

out pioneering work in the

separation of uranium

isotopes and devel-

oped Standard

Samples for

X determin-

ing the

isotopic composition of materials containing

uranium and plutonium. These materials

continue to serve the country today for the

accurate assay of reactor fuels.

After the war, breakthroughs in the fields of

electronics, and polymer research, and the

spread of spectrometric instruments brought

new demands for reference materials. By the

1950s, special hydrocarbon blends were avail-

able for calorimetry and Standard Samples

were being certified for such properties as

pH, melting point, and radioactivity. Newhigh temperature and super strength metal

alloys were needed to meet the demands of

innovations in jet aircraft and rockets.

The 50s and 60s saw an acceleration of efforts

to certify reference materials; 582 types were

available in the catalog in 1959. It was dur-

ing this period that the Bureau began to

transfer some of its efforts in reference mate-

rials to other institutions. This will be dis-

cussed in more detail in the section: "Closing

the Cycle." During the 1960s, NBS realized

that SRMs 2 were becoming increasingly

important to industry and that industrial

demand would continue to grow. The

Bureau also recognized the potential contri-

bution SRMs could make in solving measure-

ment problems in emerging areas of national

need, such as clinical and environmental

chemistry.

To appreciate the place and importance of

SRMs in the work of the Bureau at the mid-

point of its centennial requires a closer look

at events impacting the agency around the

middle of the 20th century.

2 The term "Standard Reference

Materials," and the acronym "SRM"

were introduced into use by NBS in

1965. The term and acronym were

Klater registered with the U.S.

Patent and Trademark Office.

cl Reference Materials - The First Centun/

Mid-century Turmoil

Two separate, initially very damaging, tribu-

lations fell upon the Bureau between 1948

and 1952. Eventually, the agency would

recover from these two blows with a firmer

resolve and an even stronger sense of mis-

sion. Before that happened, two directors

would face disgrace and the budget would

suffer serious decline. One of the strongest

elements of the Bureau's program was its

Standard Samples Activity, and we will see

how it was a major contributor to restoring

both fiscal and public relations health to NBS.

Edward Condon, fourth director of NBS, was

perhaps its most eminent director in terms of

scientific achievement. He was a noted theo-

retician with great insight in atomic and

nuclear physics, and provided great service to

the Nation during World War II. Prior to

leading NBS, he worked at Los Alamos on

development of the atomic bomb and served

with Chairman Lyman Briggs (third NBS direc-

tor) on Committee S-1 to directly advise

President Roosevelt on atomic and nuclear

issues, including the decision to build the

atomic bomb.

After the war, he continued to advise

President Truman and the Congress. As part

of that advice, he strongly advocated the for-

mation of the Atomic Energy Commission to

move control of nuclear activities from the

military to the civilian sector. He became a

spokesman for peaceful uses of the atom to

benefit the whole world. Neither of these

positions were popular with the military,

which had a strong post-war victory stand-

ing, or with the House Unamerican Activities

Committee. In 1948, that committee charged

Condon with being a risk to National securi-

ty. No charges were ever proved, but the

committee denied the director opportunity

to address the charges and he left NBS in

1951 to become the director of research at

(top) Aerial view of

Gaithersburg Campus (1999).

(bottom) Aerial view of

Boulder Campus (I960's).

Corning Glass, in all, it was one of the sadder

episodes of "witch hunting" seen in our

country.

The second turmoil also began in 1948, but it

peaked in 1952, thus impacting the fifth

director, Allen Astin. This cloud over the

Bureau arose from the assignment to test

many kinds of commercial products. One of

these, a battery additive named AD-X2, was

found by NBS to be ineffective. Less con-

trolled tests in other places showed some prom-

ise for the additive, so the developer (and more

significantly, his Congressman) attempted to dis-

credit NBS results. Astin was well versed in elec-

trical engineering and stood

behind the results of his tech-

nical staff through a firestorm

of Congressional hearings

and unmeasured

personal attacks.

Finally, the

Secretary of

Commerce "fired"

Astin. Now, it was

the turn of the

technical staff to

stand behind their

director.Hundreds told the

President that

they would go if

Astin went. Based

on additional data

from other

sources and the

unanimous advice

of the NBS Visiting

Committee, the

Secretary retained

Dr. Astin as direc-

tor and he served

with distinction

until retirement in

1968, foliowinc;


Table 4. NBS Funding for Selected Years

Year Appropriation ($ millions)

1946 3.6

1948 7.1

1950 8.5

1952 7.8

1954 5.7

1956 7.4

1957 8.4 + 2.8 WCF = 11.2

1958 9.7 + 2.5 WCF = 12.2

1960 201970 > 40

Comment

Condon era begins, need for war $ replacementHouse Unamerican Activities Comm. / CondonWorking Capital Fund (WCF) authorizedAstin era begins, peak of AD-X2 affair

Kelly report will shape future budgetsBudget still below 1949 level of $ 8.7 million

WCF implemented, 10yr funding crisis endedSputnik launchedFirst impact of Sputnik on budgetFinal budget developed by Dr. Astin

completion of the Boulder laboratory (1954)

and of the Gaithersburg facility (1966).

The two episodes could only adversely affect the

budgets from 1952 through 1956. More than

90% of NBS funding during the war years was

from defense sources, and that was being

reduced in peacetime. Turmoil had struck just

when it was not needed. Table 4 provides a

snapshot of the seriousness of the situa-

tion. In reading the table, it is important

to note that the budget process is slow and

usually follows impacts by about two years.

Dr. Astin's first appropriation from Congress

was for 1954, covering July 1, 1953 through

June 30, 1954, and at $5.7 million was the

smallest in the previous seven years.

A New Beginning

One response of the Secretary of Commerce

to the AD-X2 difficulty was to commission a

high- level assessment of the work and mis-

sion of NBS. The study was chaired by Mervin

Kelly, president of Bell Telephone

Laboratories. On October 15, 1953, the com-

mittee issued recommendations that would


"li

shape the Bureau for the next 35 years. The

report would become known as the Kelly

Report, and it singled out two parts of

Bureau work to praise: basic research in

metrology and the value of the standard

samples program. The Kelly Report con-

tained ten recommendations that are

grouped into three categories and presented

in Table 5, where the numbers indicate the

sequence of the recommendations as found

in the report.

It would be overreaching to say that NBS

Standard Samples rescued the Bureau at the

century's mid-point, but it would be fair to say

that they had made a very impressive mark and

again had a prime role in shaping the Bureau's

new mission. New emphasis was given to mov-

ing the development of standard samples

beyond chemistry alone. The new approach

started slowly. Then, in 1964, the Office of

Standard Reference Materials was

established and given the

responsibility for directing

all SRM activities. Table

6 provides a list of the

leaders for reference

material activities

both before and

after creation of the

new office. JfeMM^MPreviously the indi-

vidual technical divi- flficQsions had managed

separate compo- ^^^^Hnents of the SRM i^^^^lprogram with coor- ^^^^^^Hdination through

the Analytical J^^^^lChemistry Division. ^^^^HWith the establish- ^i^Hment of a new

9

Table 6. Leaders of the Standard Sample/ SRM Production Activities at NISI 1905 - 2001

Year

1905

Name

John Cain

Title

Research Associate

1918 Gustave Lundell Chief

1940 Harry Bright Chief

1950 Harry Bright andBourdon Scribner

Chief

Chief

1960 John HagueBourdon Scribner

Chief

Chief

1964 Wayne Meinke Chief

1969 J. Paul Call Chief

1979 George Uriano Chief

1983 Stanley Rasberry Chief

1991 William Reed Chief

1994 Thomas Gills Chief

2000 Nancy Trahey-Bale Chief

2002 John Rumble Jr. Chief

Organization

Chemistry Division

Analytical Methods &Standard Samples

Metal 8r Ore Analysis,

Standard Samples

Analytical ChemistrySpectrochemistry

Analytical ChemistrySpectrochemistry

Office of Standard Reference Materials




Standard Reference Materials Program





office,

a number of newthrusts were developed. Newprogram areas were identified and initi-

ated, including the start of what was to

become a major effort in developing SRMs

for clinical chemistry. For a list of some of

the key SRMs beyond the first 100, see

Appendix B.

Through the 1970s, the program had its most

productive decade in terms of the develop-

ment of both numbers and types of SRMs.

Over 600 new SRMs were certified during

that period and about 250 were discontin-

ued. By 1979, 1,060 types appeared in the

catalog. Typical of the research activity

into new SRM types in this period was a

whole array of environmental natural matrix

materials certified for inorganic constituents.

Leading the list, and arguably the most

important materials of their era, were SRM1571 Orchard Leaves, SRM 1645 River

Sediment, and SRM 1648 Urban Particulate

Matter. John Taylor directed the certification

of these materials. The river sediment was

prepared from material dredged from the

Indiana Harbor Canal, near Gary, Indiana.

Heavily loaded with toxic metals the material

served as the initial benchmark for environ-

mental studies in the field. It is also impor-

tant to note from an analytical perspective,

that these were the first environmental

matrix materials to receive extensive applica-

tion of the new isotope dilu-

tion mass spectrometry

method developed by NBS,

and which was also used to

good effect in the certification

of SRM 909 Human Serum.

During the 1980s, the many

advances in inorganic environ-

mental reference materials

were extended by the addition

of SRM certifications for organic

analytes of environmental health

concern. Some of these included

PCBs in human serum, in oil, and in

sediments. Also made available were

SRMs with certified values for a variety of

forms of dioxin, polynuclear aromatic hydro-

carbons, halocarbons, chlorinated pesticides,

and other priority pollutants.

Food-based SRMs began coming into the

inventory in the 70s and 80s with the intro-

duction of such materials as wheat flour, rice

flour, and freeze-dried bovine liver, oyster tis-

sue, and spinach leaves. The SRM efforts

toward better coverage of food types really

have seen the most progress in the 1990s,

with work being dedicated to certifying

mixed diet food materials, infant formula,

and individual foodstuffs for vitamin con-

tent. Efforts along these lines are sure to

continue into NIST's next century.

Today's Catalog

As impressive as is the history of SRM produc-

tion and certification, perhaps even more

impressive is the work summarized in the cur-

rent catalog and in the work program for

future certification. Table 7 provides the cat-

egory names that cover the approximately

1400 SRMs and other reference materials

available in the SRM catalog for 2001, avail-

able under the NIST home page on the World

Wide Web as well as in printed form.


Wide dissemination of information on avail

ability, including exhibits at 5 to 10 confer

ences each year, helps the

program distribute more

than 35,000 units of

material to about 10,000

customersApproximately one-third

of each year's sales are

delivered abroad.

Closing the Cycle

As many types of reference

materials matured and NIST

interests turned to other

technologies, efforts have

been made to find institu-

tions willing to receive trans-

fer of the materials and

responsibilities. This is essen-

tial to permit reallocation of

scarce resources to fund new efforts.

During the 1 950s and 60s, some of the first of

these transfers took place. The extensive

hydrocarbon blend project was transferred

to the American Petroleum Institute. Color

and fading SRMs were transferred to the

American Association of Textile Chemists and

Colorists, and viscosity materials went to

Carnegie-Mellon University. During the

1980s, in part for security reasons, the SRMs

for uranium and plutonium were transferred

to the New Brunswick Laboratory of the US

Department of Energy located at Argonne

National Laboratory. At the beginning of the

1990s, NIST was closing out its work on rub-

ber compounding so about a dozen types of

rubber compounding, SRMs were transferred

to ASTM. These are a few of many examples

of "passing the baton" on reference materi-

als that NIST can no longer support.

Not all the transfer efforts have involved

actual movement of the materials. Most of

the metal materials that have figured so

Table 7. SRM Categories for 2001

Health and Clinical

industrial Hygiene

Environmental

Food and Agriculture

High Purity Materials

industrial Materials

Engineering Materials

Physical Properties

Radioactivity

heavily in the early devel-

opment of the Standard

sample and SRM pro-

grams, have remained at

NIST, but much of the certification effort on

renewal lots is only undertaken by laborato-

ries organized in cooperation with ASTM. It

is highly likely that the trend will be for NIST

to continue to seek partners in industry, uni-

versities, or other government agencies to

provide homes for SRMs and RMs being

closed out at NIST.

Benefit/Cost

The annual cost each year for all types of

measurements in the United States is counted

in the hundreds of billions of dollars. A small

view of the scale and vigor of the activity in

analytical chemistry alone is seen each year at

the Pittsburgh Conference on Analytical

Chemistry and Applied Spectroscopy, where

about 30,000 conferees gather, they represent

perhaps a tenth of their colleagues working in

the field. Those who have attended this con-

ference for many decades will recognize the

many changes in the field that have brought

significant improvements in effectiveness and

efficiency to most types of chemical analysis.

The driving forces behind these changes have

included the rapid and far-reaching develop-

ment of instrumentation, the improvement of


analytical methods, and the avail-

ability of Standard Reference

Materials from NIST and sec-

ondary suppliers.

It is not hard to calculate that an

SRM contribution to measure-

ment improvement, even as

small as 0.1 %, would save com-

panies which measure hundreds

of millions of dollars each year -

easily justifying the approxi-

mately $10 million spent annual-

ly to buy SRMs. Client demandfor ever increased numbers of

types provides a qualitative indi-

cator of the program benefits.

The demand requires careful pri-

oritization, for it greatly exceeds

each year's SRM budget. Table 8 summa-

rizes the approximate number of SRM types

available at ten-year intervals. The table

data are not exact since no hard data were

recorded for most of the intervals. However,

several sources have been studied and the

values are probably dependable, with an

uncertainty of less than 10 % of each value.

Reasons for the ambiguity include discontin-

uation of SRMs (with perhaps 1000 types hav-

ing been discontinued over the history of the

program) and an uncertain number of mate-

rials listed in catalogs being out of stock at a

given time. Additionally, SRMs have not

been numbered sequentially, complicating

historical counts.

What is harder to quantitate is the social con-

tribution made by SRMs. In a study by the

Research Triangle Institute on the economic

impact of SRMs for sulfur in fossil fuels, three

economists led by Sheila Martin determined

that the group of SRMs had a benefit/cost

ratio of 113, and a social rate of return of

more than 1,050 %. Similar conclusions have

been reached at other times and in other

studies with regard to a variety of SRMs.

While not as quantifiable, there are major

ur 11^

Ma

benefits to

people dependent on good clinical measure-

ments; for example, the child whose epileptic

seizures are better controlled by measure-

ments improved with SRMs. In another

example, cholesterol measurement uncer-

tainties have been reduced from 20 % in the

1970s to 5 % in the 1990s, again with the

help of SRMs. It is clear that customers'

demands for more and better SRMs are unre-

lenting. Despite the common complaint

"SRMs cost too much," customers continue to

buy them in quantities adequate to fund

future certification programs.

Table 8. Approximate Number of SRM types

Available by Decade

Year Number Year Number

1910 20 1960 400

1920 50 1970 600

1930 90 1980 1100

1940 200 1990 1200

1950 250 2000 1300


Collaboration Around the World

Especially over the last five decades, the

Bureau has nurtured strong ties tor interna-

tional cooperation. About 25 years ago,

the International Organization for

Standardization (ISO) accepted as a Council

Committee, a group to work on reference

materials. The committee was first referred

to as REMPA and very quickly had a change in

name to ISO Committee on Reference

Materials (REMCO). Strong impetus for its

founding and early success was supplied by

NBS staff members such as Bill Andrus, Paul

Call, and George Uriano. REMCO has become

the focus for defining the terminology and

practices of reference material certification

and use.

NIST has participated in many bilateral and

multilateral cooperations. Some of these

have had a goal of certification of a specific

SRM or groups of SRMs, while others have

been oriented toward helping other coun-

tries get started in the field. As an example

of the latter, NIST hosted approximately 200

chemists from China over the first 15 years

following renormalization of relations

between the two countries. Analysis of SRMs

was part of the effort for many of the

chemists. Some of them, on return to China,

established a very vital program in produc-

tion of reference materials. On a

smaller scale, cooperative

projects have been s

with Mexico folio

the implementation

of the North

American Free

Trade Agreement and agreements for coop-

eration in metrology. Additional efforts have

been carried out with France, the United

Kingdom, Germany, Japan, Egypt, Poland,

and several other countries.

Some of the most effective collaborations are

those aimed at gathering data to characterize

proposed new reference materials. In recent

years these have included many countries

contributing to the development of SRMs. Afew examples include the certification of

infant formula and mixed diet SRMs, and also

a large suite of food RMs from Canada. Other

efforts have included contributions from most

of the world's industrialized countries. Anearlier example occurred in the late 1970s.

NBS partnered with 70 individuals from 22

organizations in the U.S. copper industry and

ASTM to develop a series of unalloyed copper

SRMs. Robert Michaelis, Jerry Hust, and Lynus

Barnes directed the effort which received not

only a large measure of U.S. industrial sup-

port, but also the contribution of data from

Canada, South Africa, South America, and the

European contributors.

Conclusion

The aim of this brief account has been to

highlight a few of the many contribu-

tions that NBS-NIST has made

through the

certifica-

ference Materials - The First Century

and distribution of reference materials. The

selection of examples cited only begin to

probe the surface and cannot do real justice

to the program in its entirety over almost 100

years. Many chemists will, however, relate to

the great feeling of success that comes when

analyzing an SRM from NIST and obtaining

the certified values or discovering a disagree-

ment, thereby preventing the propagation of

an error!

Standard Samples and SRMs have been

among the most widely known and distrib-

uted measurement artifacts of all the

NBS/NIST contributions, with several million

units having been circulated in the first 100

years. Few are the scientists around the

world who have not heard of SRMs and the

Nisr ,

Standard I

Reference jBMaterials fi(301)975-6776

™

value they provide for validating a method or

calibrating an instrument. By promoting and

sharing the ideas and technologies of reference

material development, the Bureau has been a

good neighbor in the world community.

Standard Samples and SRMs have represent-

ed some of the finest efforts produced by

NIST. By successfully solving material-related

problems and bringing attention to those

successes, the work on reference materials

has had a major effect on the development

of the early Bureau's selection of work pro-

grams and ultimately its character as a world-

class metrology organization. It has been an

exciting century for the field of reference

materials in support of analytical chemistry

and the other sciences. Perhaps it will be seen

in another 100 years as a

worthy introduction to

the even greater things

that are yet to come for

NIST SRMs.

I www.nistgov/srm

For those inclined to spec-

ulate about the future, a

few of the author's

notions are tabulated in

Appendix C. The only

certainty about them is

that they are uncertain.

They are most likely to

be seen in retrospect as

too conservative.


Appendix A Cooperation With ASTM in Standard Reference

Material Development

The NBS/NIST reference materials program

has, since it began to develop reference mate-

rials in 1904, benefited from close coopera-

tion with many of the nation's finest technical

societies and associations. It is clear today

that without this cooperation, the program

would either never have started or would be

vastly different and probably greatly dimin-

ished in size and scope. None of the alliances

has been more far reaching and had greater

impact than the one with the American

Society for Testing and Materials (ASTM).

Starting before the second world war, the

cooperation has arranged for the shared

development of more than 1000 Standard

Samples and Standard Reference Materials.

Formal Research Associate Programs have

posted ASTM staff at NIST to participate

directly in the preparation and measurement

of candidate materials and, perhaps even

more importantly, to arrange for the techni-

cal assistance of many contributors from hun-

dreds of industrial laboratories. Today, ASTME01.94, Subcommittee on Development of

Reference Materials for the Chemical Analysis

of Metals, Metal-Bearing Ores and Related

Materials, meets semiannually to prioritize

requests to NIST for new and renewal refer-

ence materials and to cooperate in their

development.

In 1987, the author prepared a list of selected

instances where SRMs are specified for use in

ASTM technical standards. The list is by no

means complete (for example ASTM D02.SC3,

Subcommittee on Elemental Analysis,

recently included SRM 1848 "Lubricant

Additive Package" in new standards

for motor oil test methods), but is

given below to indicate the scope

of SRM inclusion in ASTM stan-

dards.

During its first century, NIST has

provided technical staff expertise

in ASTM, filling as many as 800 com-

mittee assignments in some years.

Several staff members have served as

directors on the ASTM Board. The former

chief of the Standard Reference Materials

Program, Nancy Trahey-Bale, was one of

those, having served as treasurer and later as

chairman of the Board of Directors for ASTMin 1993.

INTERNATIONAL

Standards Worldwide

Standal Materials - The First Century 21

Selected Examples of SRM Incorporation in ASTM Standards (as of 1987)

ASTMSTANDARD TEST NIST SRM

C 204 Cement Fineness (Blaine) 114n Portland Cement

C 115 Cement Fineness (Wagner) 114n Portland Cement

C430 Sieve Residue 114n Portland Cement

C 336 Glass Annealing and Strain Points 711 and 717 Glass Viscosity

C338 Glass Softening Points 711 and 717 Glass Viscosity

C657 Glass Electrical Resistivity 624 Glass Electrical Resistivity

C770 Glass Stress Optical Coefficient 708 and 709 Glass

C829 Glass Liquidus Temperature 773 Glass Liquidus Temperature

D 1238 Melt Flow Rate (Plastic) 1475 and 1476 Polyethylene

D 1505 Density (Plastic) 1475 and 1476 Polyethylene

D 1434 Gas Transmission Rate (Volumetric) 1470 Polyester Film

D 1434 Gas Transmission Rate (Manometric) 1470 Polyester Film

D 3985 Gas Transmission Rate (Coulometric) 1470 Polyester Film

D 1646 Mooney Viscosity 388m Butyl Rubber

D 2268 Chemical Analysis of Fuels 1816a isooctane

D 3177 Sulfur Analysis in Coal and Coke 2682-2685 Sulfur in Coal

D 4239 Sulfur Analysis in Coal and Coke 2682-2685 Sulfur in Coal

D 2795 Analysis of Coal and Coke Ash Soda Feldspar

E 27 Analysis of Zinc and Zinc Alloys 94c Zinc Base Alloy

E 129 Analysis of Thermionic Nickel 671-673 Nickel Oxide

E 322 Analysis of Steels and Cast Irons numerous steel/iron SRMs cited

E 539 Analysis of 6AI-4V Titanium Alloy 173 and 654a Titanium Alloy

E 162 Flame Spread Index 1002c Surface Flammability

E 648 Critical Radiant Flux 1012 Flooring Radiant Panel

F 746 Pitting and Crevice Corrosion 1890-1891 Crevice Corrosion


Appendix B Key NBS Reference Materials Beyond the First 100

Numbering of Standard Samples and

Standard Reference Materials has been

assigned according to several different sys-

tems during the first century of production

and certification. Almost all of the first 100

SRMs were completed before 1930 and

assigned numbers more or less in sequence,

with the exception of the first four "standard

samples" (as was discussed in the main text).

Occasionally a number was reserved for a

certain SRM, such as 85 for aluminum alloy

(Duralumin) first issued in 1943, that had a

delayed issue or was not issued at all. In a

few cases, numbers for unissued materials

and SRMs that were issued but discontinued

have been reused for different materials.

Current practice retires the numbers of dis-

continued materials. Typically, when a given

lot of material for an SRM is exhausted and

replaced with a new lot, new certification

measurements and a new certificate are

required. The new lot of the SRM retains its

numerical designation and a lower case let-

ter is appended or changed to denote the

lot. For example, SRM 916a Bilirubin is the

first reissue (second material lot) of SRM 916

Bilirubin, while SRM 955b Lead in Blood is

the third lot of that material.

The table that follows sketches the development

of SRM types over time by listing the date of ini-

tial issue for selected key materials. The list is

intended only to be representative as it includes

but a small percentage of all materials issued.

Selection for the list typically indicates the SRM is

an early member of a given material type.

Selected Key NBS/NIST Reference Materials Beyond the First 100

SS/SRM

102

103

112

113

119

TITLE

Silica Brick

Chrome Refractory

Silicon Carbide

Zinc Concentrate

Chromel P

DATE

1932

1934

1937

1941

1935

APPLICATION

Composition

Composition

Composition

Composition

Thermometry

120

136

140

147

154

Phosphate Rock

Potassium Dichromate

Benzoic Acid

Triphenyl Phosphate

Titanium Dioxide

1939

1948

1942

1969

1943

Composition

Oxidimetric

Microcombustion

Microanalytical

Composition

160

162

164

165

173

Stainless Steel 19Cr-9Ni-3Mo

Ni-Cu Alloy

Mn-AI Bronze

Glass Sand

Titanium Base Alloy (6AI-4V)

1949

1949

1951

1948

1957

Composition

Composition

Composition

Composition

Composition


(Continuation of Table)


SS/SRM TITLE DATE APPLICATION

187 Borax pH Standard 1947 pH Standard

303 Burnt Sienna 1944

330 Copper Ore Mill Heads 1973 Composition

331 Copper Ore Mill Tails 1973 Composition

343 Stainless Steel 16Cr-2Ni 1962 Composition

349 Waspalloy 1959 Composition

475 Optical Microscope Linewidth Measure 1981

480 Electron Microprobe Standard (W-20Mo) 1968 Composition

482 Gold-Copper Wires for Microprobe 1969 Composition

484 Scanning Electron Microscope Mac|nication 1977 Length

485 Austenite in Ferrite 1970 Composition

592 Hydrocarbon Blend No. 1 1961 Composition

600 Bauxite 1988 Composition

601 Spectrographic Aluminum 1951 Composition

610 Trace Elements in Glass Matrix 1970 Composition

620 Soda Lime Flat Glass 1972 Composition

621 Soda Lime Container Glass 1975 Composition

623 Borosilicate Glass 1976 Composition

633 Portland Cement 1974 Composition

640 Silicon Powder for X-ray Diffraction 1974 Lattice Pattern

671 Nickel Oxide 1960 Composition

674 X-ray Powder Diffraction 1983 Intensity

679 Brick Clay 1987 Composition

680 High Purity Platinum 1967 Composition

702 Light Sensitive Plastic Chip 1966 Fading

705 Polystyrene 1963 Molecular Weight

740 Zinc Freezing Point 1970 Temperature

762 Magnetic Moment * Nickel Disk 2000 Magnetic Moment767 Superconductive Fixed Point 1974 Temperature

772 Magnetic Moment - Nickel Sphere 1978 Magnetic Moment

781 Molybdenum - Heat Capacity 1977 Heat Capacity

870 Column Performance for LC 2000 Efficiency

877 Chiral Selectivity for LC 2000 Selectivity

909 Human Serum (Clinical) 1980 Composition

911 Cholesterol (Clinical) 1967 Composition

912 ^ Urea (Clinical) 1968 Composition

913 Uric Acid 1968 Composition

914 Creatinine 1968 Composition

916 Bilirubin 1971 Composition

927 Bovine Serum Albumin (Total Protein) 1977 Composition


(Continuation of Tabfe)

Selected Key NBS/NiST Reference iVIaterials Beyond the First 100


930 Glass Filters for Spectrophotometry 1971 Transmittance

934 Clinical Laboratory Thermometer 1974 Temperature

945 Plutonium iVIetal 1971 Assay

946 Plutonium isotopic 1971 Composition

955 Lead in Blood 1984 Composition

968 Fat Soluble Vitamins in Human Serum 1989 Composition

987 Assay-lsotopic Strontium 1971 Assay & Composition

1001 X-ray Film Step Tablet 1973 Optical Density

1003 Calibrated Glass Spheres 1965 Length

1008 Photographic Step Tablets 1971 Optical Density

1010 Microcopy Resolution Test Charts 1963 Resolution

1013 Portland Cement 1962 Composition

1083 Wear Metals in Lubricating Oil 1985 Composition

1244 Inconel 600 1984 Composition

1246 Incoloy 800 1984 Composition

1261 AISI 4340 Steel 1970 Composition

1321 Coating Thickness - Nonmagnetic on Steel 1988 Length

1387 Coating Weight - Gold on Nickel 1985 Length

1400 Bone Ash 1992 Composition

1470 Polyester Film - Gas Transmission 1978 Transmission

1475 Linear Polyethylene 1969 Molecular Weight

1479 Polystyrene 1981 Molecular Weight

1491 Aromatic Hydrocarbons in Hexane/Toluene 1989 Composition

1492 Chlorinated Pesticide in Hexane 1989 Composition

1511 Multi-Drugs of Abuse in Freeze-dried Urine 1994 Composition

1515 Apple Leaves 1991 Composition

1521 Boron-doped Silicon Slices for Resistivity Meas. 1978 Resistance

1523 Silicon Resistivity for Eddy Current Testers 1985 Resistance

1544 Fatty Acids 8i Cholesterol in Frozen Diet 1996 Composition

1546 Meat Homogenate 2000 Composition

1547 ^^Peach Leaves 1991 Composition

1548 Total Diet 1990 Composition

1549 Non-fat Milk Powder 1984 Composition

1563 Cholestrol & Fat-Soluble Vitamins in Coconut Oil 1987 Composition

1566 \\Oyster Tissue 1979 Composition

1567 Wheat Flour 1978 Composition

1568 Rice Flour 1978 Composition

1570 Trace Elements in Spinach 1976 Composition

1571 Orchard Leaves 1971 Composition

1577 ^^ovine Liver 1972 Composition





1579 Powdered Lead Based Paint 1973 Composition

1580 Ornani^c in CliJilo OilWl^ClKII^S III Allelic Wll 1980 Composition

1581 PoiychloriiidtiGcl BiphGnyls in Oils 1982 Composition

1582 Petroleum Crude Oil 1984 Composition

1583 ClorindtGci Pesticides in 2r2f4~'trinie'tliylpentdne 1985 Composition

1584 Priority Pollutant Phenols in Methanol 1984 Composition

1588 Orânics in Cod Liver Oil 1989 Composition

1589 Polychiorinated Biphenyls in Human Serum 1985 r'omnncif'ion\>UIII|JU3l IIUII

1590 9iaijiiizea Wine 1980 Alcohol Content

1598 Inorganic Constituents in Bovine Serum 1989 Composition

1599 Anticonvulsant Drug Level Assay 1982 Assay

1601 Carbon Dioxide in Nitrogen 1973 Composition

1604 Oxygen in Nitrogen 1968 Composition

1610 U%/rli*nÂvhrkn in Airnyui vvdi uvrii iii nii 1969 ^nmnncitinn\h\JIiI|JU9I IIUII

1614 1985 Composition

1617 Sulfur in Kerosine 1988 Composition

1619 Sulfur in Residual Fuel Oil 1981 Composition

1625 Ciilfiir ninvirlo PAVmoAtinn TiihoiÛIIUl IÎUAIUC rV?! IIICCILIUII lUMV? 1970 rkmnncition^VIII|^V9l llVf 1

1630 TvAfo lUloffiii^ in aaIiidwc iviciûiy III v«wcii 1971 Composition

1633 Traf*o Fickinon'I'C in âaI Plu Acliiidvc ciciiiciiLs III v>ucflB " 'y '^^1 1974 ^nmnocitinnÛIII|JV9l LIUll

1634 '"^ Trace Elements in Fuel Oil 1978 Composition

1636 Lead in Reference Fuel (Gasoline) 1975 ^nmnocitinnÛlll|JU9l LIUll

1640 Trace Elements in Natural Water 1997 Composition

1641 ivitfiLUiy III WdLtfi 1974 ^nmnrhcitinn^VIII|JW9l LIVII

1643 Trar*o Flomontc in lAfAtoi*iidw cidiivjiiLa III wdLisi 1977 Composition

1645 ^ River Sediment 1978 Composition

1646 1982 Composition

1647 Prinritv Pnllutant PAHc 1981 Composition

1648 WTfJan rclrXICUIaXe IVIcitlcr 1978 r^nmnncition

1649 Urban Dust / Organics Composition

1650 Diesel Particulate Matter 1985 Composition

1659 Methane in Air 1976 Composition

1661 Sulfur Dioxide in Nitrogen 1976 Composition

1669 Propane in Air 1973 Composition

1677 Carbon Monoxide in Air 1974 Composition

1683 Nitric Oxide in Nitrogen 1974 Composition

1745 Indium Freezing Point 1998 Temperature

1761 Low Alloy Steel 1985 Composition

1866 Bulk Asbestos - Common 1988 Composition

1895 Nickel Microhardness - Knoop 1984 Hardness




SS/SRM TITLE PATE APPLICATION

1896 Nickel IVIicrohardness - Vickers 1992 Hardness

1920 Near Infrared Reflectance Wavelength 1986 Wavelength

1921 Infrared Transmission Wavelength 1984 Wavelength

1922 Liquid Refractive Index - Mineral Oil 1999 Refractive Index

1930 Glass Filters for Spectrophotometry 1987 Transmittance

1941 Organics in Marine Sediment 1989 Composition

1945 Organics in Whale Blubber 1994 Composition

1951 Cholesterol in Human Serum (Frozen) 1988 Composition

I960 Nominal 10 Fm Dia. Polystyrene Spheres 1985 Length

1968 Gallium Melting Point 1977 Temperature

1974 Organics in Mussel Tissue 1990 Composition

2003 Aluminum on Glass - First Surface Mirror 1971 Reflectance

2030 Glass Filters for T^ansmittance 1976 Transmittance

2031 Metai-on-Quartz Filters Spectrophotometry 1984 Transmittance

2069 Scanning Electron Microscope Performance 1983 Efficiency

2071 Sinusoidal Roughness Specimen 1989 Roughness

2084 CMM Probe Performance 1994 Length

2092 Low-Energy Charpy V-Notch Test 1989 Energy

2109 Chromium (VI) Speciation Stan'rd Solution 1992 Composition

2121 Spectrometric Standard Solutions 1984 Composition

2135 Nickei/Cromium Thin-Film Depth Profile 1985 Length

2261 Chlorinated Pesticides in Hexane 1992 Composition

2287 Ethanol in Reference Gasoline 1995 Composition

2294 Reformulated Gasoline 1998 Composition

2381 Morphine 8i Codeine in Freeze-dried Urine 1992 Composition

2383 ' Baby Food Composite 1997 Composition

2390 DNA Profiling Standard 1992 Structure

2392 Mitochondrial DNA Sequencing - Human 1999 Structure

2415 Battery Lead 1991 Composition

2416 Bullet Lead 1988 Composition

2524 Optical Fiber Chromatic Dispersion 1997 Dispersion

2526 (111) p-Type Silicon Resistivity 1983 Resistance

2531 Etiipsometric Parameters - Si02 on Silicon 1992 Length

2541 Silicon Resistivity - 0.01 ohm • cm Level 1997 Resistance

2556 Used Auto Catalyst 1993 Composition

2567 Catalyst Package for Lubricant Oxidation 1992 Composition

2570 Lead Paint Film 1999 Composition

2583 ' Trace Elements in Indoor Dust 1998 Composition

2670 Toxic Metals in Freeze-dried Urine 1993 Composition

2676 Metals on Filter Media 1975 Composition





2682 Sulfur in Coal 1982 Composition

2694 Simulated Rainwater 1985 Composition

2710 Montana Soil 1992 Composition

2712 Lead in Reference Fuel (Gasoline) 1988 Composition

2782 Industrial Sludge 1998 Composition

2810 Rockwell C Scale Hardness - Low Range 1998 Hardness

2811 Rockwell C Scale Hardness - Mid Range 1998 Hardness

2812 Rockwell C Scale Hardness - High Range 1998 Hardness

3087 Metal on Filter Media 1990 Composition

3101-69 Element Solution for Spectrometry 1986 Composition

3171 Multielement Mix A Standard Solution 1988 Composition

3190 Aqueous Electrolytic Conductivity 1990 Conductivity

3200 Magnetic Tape - Computer Amplitude 1969 Signal Amplitude

4200B Point Source Radioactivity 1965 Radioactivity

4201 Gamma Ray Niobium-94 1965 Radioactivity

4203B Cobalt-60 Gamma Ray Point Source 1967 Radioactivity

4350 Environmental Radioactivity - River Sediment 1975 Radioactivity

4351 Environmental Radioactivity - Human Lung 1982 Radioactivity

4352 Environmental Radioactivity - Human Liver 1982 Radioactivity

4353 Environmental Radioactivity - Rocky Flats Soil 1981 Radioactivity

4355 Environmental Radioactivity - Peruvian Soil 1982 Radioactivity

4356 Ashed Bone 2000 Radioactivity

4357 Environmental Radioactivity - Ocean Sediment 1997 Radioactivity

4408-27 Radiopharmaceuticals (Short Half Lives) 1960's Radioactivity


Appendix C Past and Future Driving Forces on Reference

Material Production

The following table is the author's attempt

to crystalize the most powerful driving forces

on the selection and production of reference

materials over the first century of NIST oper-

ation. On less stable ground, guesses are

made at how new forces may develop over

the course of the next century, thus shaping

the SRM program in years to come.

TIME FRAME1901 - 1924

1925 - 1949

1950 - 1974

1975 - 2000

Speculation:

2001 - 2024

2025 - 2049

2050 - 2074

2075 - 2100

DRIVING FORCESAutomotive Age Explodes

Industrial Progress

WW I

Depression

Industrial Scale-up

WW II

Korea

Space Race

Vietnam

Human NeedsInfo Age Explodes

Economic Competition

Biotech Revolution

Infrastructure Reconstruction

New (Fusion?) Energy AgeNanotechnology Breakthroughs

Large-scale Environmental

Reconstruction

Space Colonization

SS/SRM RESPONSESMetals, Ores, and CementThermometry/Calorimetry

Sucrose

Primary Chemicals

Glass and Ceramics

Aluminum Alloys

High Strength Alloys

High Temperature Alloys

Metrology & Semiconductor

Environmental & Clinical

Food & Agriculture

Fuels, Oils & Engine Wear

New Suite of DNALab on Chip Validators

Many SRMs become NTRMs(NIST traceable reference materials)

Ultrastrength Materials

Nanometrology

Ultra Complex Natural

Matrix Materials

New Fuels, Foods, Materials

NIST's Numerically

Controlled

Diamond Turning

Machine used to

manufacture

RM 8240

Standard Bullets

with identical sig-

natures.

- : Materials - The

Standard Reference Materials : the first century€¦ · NIST260-150...

Documents

Transcript of Standard Reference Materials : the first century€¦ · NIST260-150...